Product obtainable by treating wool fat with a sulphonating agent and process of preparing the same



v Patented Oct. 1930 (UNITED STATES PATENT OFFICE GUSTAV MAUTHE, OFCOLOGNE-EOLWEIDE'AN D ALFRED THAUSS, Oi CQIDGNE-DEU'IZ,

GERMANY, ASSIGNORS TO GENERAL ANILINE WORKS, ING., OF NEW YORK, N. 'Y.,A

CORPORATION OF DELAWARE FBODUGT'OBTAINABLE BY TREATING WOOL RAT WITH A.SULPHONATING GENT AND PROCESS OF PREPARING THE SMIE No Drawing.Application filed February 24, 1928, Serial No. 256,806, and in GermanyMarch 1, 1927.

The present invention relates to new products obtainable by treatingwool fat with a sulphonating agent and to a processof pre- I solidmasses are obtainable which on boiling with water form emulsions whichare stable,

even when the reaction of the emulsion is acid. They form clearsolutions on the addition of alkali to the emulsion and are easilysalted out from either the alkaline neutral or acid medium by theaddition of a neutral salt.

It is tobe'understood that the term wool fat is intended to includecleaned wool fat as well as raw wool fat, which still contains variableamounts of free fatty acid.

We prefer to effect the sulphonation by reacting with sulfuric acidmonohydrate, chlorosulfonic acid or a mixture of them in the presence ofa phenol on wool fat for a. prolonged time, between a few hours and twodays and at a temperature from about 5 to 40 C. The sulphonation canalso be carried out by dissolving the wool fat-phenol mixture in asuitable organic solvent which 7 is indiiferent to sulphonating agents,such as chloro-hydro-carbons, hydro-aromatic compounds, carbon disulfideetc. and adding the. sulphonating agent to this solution. this lattercase on working up semi-solid friable masses are obtainable. 2'

Our new products are capable of'varied application for example in thetextile and leather industries, y Y

The followingexamples will illustrate our invention without limiting itthereto:

Ewample 1;60 parts byvweight of ordinary commercial neutral wool fat and30 parts by weight of phenol are stirred at 20 to 30 C. with 70 parts byweight of sulfuric acid monohydrate and then gradually 70 parts byweight of chloro-sulfonic acid, are added" stirring being continued forseveral hours. Thesulphonation mixture after standing for day ispoured'upon a mixture of 100 parts by weight of ice and parts by weightof a saturated aqueous sodiuinsulfate solution.

wool fat and 25 parts by rated The resulting'mass is kneaded andseparated from the aqueous acid solution. It is then stirred with 300parts of water and almost completely neutralized with caustic soda lye.The remainder of the free acid is neutralized with sodium acetate andthe mixture is heated for a considerable time to about 90 (1.,

whereupon it separates into two layers. Af-

ter cooling the upper layer represents a butter-like mass, whichdissolves in hot water to an opalescent solution, which exhibits weaklyacid reaction. Acetic acid and dilute mineral acid do not causeprecipitation, the latter only cause a color change of the emulsion fromyellow to greyish green. The colloidal solutions of the substance areeasily salted out.

Ewample 2T-100 parts by weight of heutral wool fat and 35-parts byweight of phenol are dissolved with gentle warming in 100 parts byweight. of tetrachloroethane and to the solutionare added 200 parts byweight of sulfuric acid monohydrate at about 20 C.

After standing for about 24 hours the ice cold mixture is poured into1000 parts by weight saturated aqueous sodium chloride solution. Theresulting fat-like mass is separated and then freed-from the excess ofsulfuric acid by repeated washing with salt solution. A semi-solid massis thus obtained, which dissolves in warm water to a clear opalescentweakly acid reacting solution. 1

Example 31-50 parts by weight of neutral weight of phenal are dissolvedin 25 parts by weight of cyclohexane and to the solution are added 90parts by weight about 10 C. The-mixture is left to stand for of sulfuricacid monohydrate at some time at ordinary temperature and thenpouredinto 500 parts by wei ht of cold satuaqueous sodium c ridesolution,

stirred well and the resulting semi-solid mass is separated. The productcan be completely freed from the. excess of acid by repeated washing.Thefri able, soft mass thus obtainof phenol and then the melt is stirredat a' 4-60 parts byweight of raw.

95, able is .soluble in warm water g vingaclear about 5-40 acid byrepeated solvingin water and salting out and is obtained as a brownsubstance,

which is semi solid in the cold and soluble in water to a clearsolution.

We claim:

1. The process which comprises treating wool fat with a sulphonatingagent in the presence of a suitable phenol.

2. The process which comprises treating wool fatwith a sulphonatingagent in the presence of a suitable phenol at a temperature fromabout540 C.

3. The process which comprises treating wool fat with a sulphonatingagent in the presence of phenol.-

4. The process which comprises treating wool fat with a sulphonatingagent in the presence of henol at a temperature from about 540 l 5. Theprocess which comprises treating wool fat with a sulphonating agent inthe presence of a suitable phenol and an organic solvent.

6. The process which comprises treating wool fat in the presence of asuitable phenol and a suitable organic solvent with a sulphonating agentat a temperature from 7. The process which comprises treating wool fatin the presence of phenol and a suitable organic solvent with'asulphonating agent. I v

8. The process .which comprises treating wool fat in the presence ofphenol and a suitable organic solvent with a sulphonati agent at atemperature from about 540 9. The process which comprises treating woolfat in the presence of a suitable phenol for several hours with sulfuricacid monohydrate at a temperature from about 540 C;

10. The process which comprises treating wool fat in thepresence ofphenol for about 24 hours with sulfuric acid monohydrate at a temerature from about 1520 C.-

11. he process which comprises treating wool fat in the presence ofphenol and a suitable organic solvent for several hours with sulfuricacid monohydrate at a temperature from about 540 C.

12. Theprocess which comprises treating wool fat in the presence ofphenol and a sulfuric acid monohydrate at a temperature of about 20 C.

14. The new products obtainable by treating wool fat with a sulphonatingagent in the presence of a henol being semi-solid and friable massesfarming on boiling with water stable emulsions which form clearsolutions when rendered alkaline, said products being salted out fromtheir neutral alkaline or acid solutions by the addition of a neutralsalt.

15. The new product obtainable by treating neutral wool fat withsulfuric acid monohydrate in the presence of phenol being a semi-solidfriable mass which on boilmg with water forms a stable emulsion whichforms a clear solution when rendered alkaline, said product being saltedout from its neutral alkaline and acid solutions by the V addition of aneutral salt.

In testimony whereof we have hereunto

